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目的:建立反相高效液相色谱法测定氯高铁血红素原料药的有关物质。方法:采用ODS色谱柱(150 mm×4.6 mm,5μm);以甲醇-乙腈-0.05 mol.L-1醋酸铵缓冲液(冰醋酸调pH 3.0)-吡啶(31∶31∶38∶0.4)为流动相;检测波长为399 nm;流速1.0 mL.min-1;柱温30℃。结果:氯高铁血红素浓度在0.0205～0.1025μg.mL-1范围内,浓度与主要杂质峰面积呈良好的线性关系(r=0.9999),重复性试验中单个杂质含量的RSD为1.8%(n=6)。结论:该方法简便、快速、准确且重复性好,可作为氯高铁血红素原料药的有关物质控制方法。
Objective: To establish a reversed-phase high performance liquid chromatographic method for the determination of related substances of hemin. METHODS: ODS column (150 mm × 4.6 mm, 5 μm) was used. The column was eluted with methanol-acetonitrile-0.05 mol·L-1 ammonium acetate buffer (adjusted to pH 3.0 with glacial acetic acid) Mobile phase; detection wavelength was 399 nm; flow rate was 1.0 mL.min-1; column temperature was 30 ℃. Results: The concentration of hemin was in the range of 0.0205-0.1025μg.mL-1, and the linear relationship was obtained between the concentration and the main impurity peak area (r = 0.9999). The RSD of single impurity in the repeated test was 1.8% (n = 6). Conclusion: The method is simple, rapid, accurate and reproducible. It can be used as a related substance control method for hemin.